WO2023162593A1 - Dispositif et procédé de traitement des eaux - Google Patents

Dispositif et procédé de traitement des eaux Download PDF

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Publication number
WO2023162593A1
WO2023162593A1 PCT/JP2023/003009 JP2023003009W WO2023162593A1 WO 2023162593 A1 WO2023162593 A1 WO 2023162593A1 JP 2023003009 W JP2023003009 W JP 2023003009W WO 2023162593 A1 WO2023162593 A1 WO 2023162593A1
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Prior art keywords
water
hypochlorite
treated
urea
added
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PCT/JP2023/003009
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English (en)
Japanese (ja)
Inventor
優仁 栩内
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栗田工業株式会社
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Publication of WO2023162593A1 publication Critical patent/WO2023162593A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens

Definitions

  • the present invention relates to a water treatment apparatus suitable for efficiently decomposing and removing urea in water to produce and supply ultrapure water with a low TOC concentration, and a water treatment method using this water treatment apparatus.
  • ultrapure water production equipment that produces ultrapure water from raw water such as city water, groundwater, and industrial water basically consists of a pretreatment device, a primary pure water production device, and a secondary pure water production device.
  • the pretreatment device is usually composed of a flocculation device, a flotation device, a filtration device, and the like.
  • the primary pure water production device is composed of one or two reverse osmosis membrane devices and mixed bed ion exchange devices, or ion exchange devices and reverse osmosis membrane devices
  • the secondary water purification device is composed of low-pressure ultraviolet oxidation It consists of a device, a mixed bed ion exchange device and an ultrafiltration membrane device.
  • the ultrapure water to be supplied is required to be of high purity with a sufficiently reduced TOC. It is extremely important to remove urea in an ultrapure water production system because it causes an increase in TOC concentration.
  • Patent Literature 1 discloses treatment by a water treatment apparatus as shown in FIG.
  • a sodium hypochlorite (NaClO) adding means 23 and a sodium bromide (NaBr) adding means 24 as a chemical adding mechanism are connected in the middle of a raw water W supply pipe 22.
  • a mixing device 25 and a reaction tank 26 are provided on the downstream side of this, and a sodium bisulfite (NaHSO 3 ) addition mechanism 27 as a reducing agent is connected to the downstream side of this, and this treated water W1 is transferred to the primary pure water device It can be supplied to post-processing such as.
  • a urea meter 28 is provided on the upstream side of the sodium hypochlorite (NaClO) addition mechanism 23 of the supply pipe 22 of the raw water W, and the urea meter 28 is controlled by a control means (not shown). Based on the measured value of the total 28, the sodium hypochlorite adding means 23 and the sodium bromide adding means 24 can be controlled.
  • the chemical necessary for decomposing urea is exceeded.
  • urea can be stably and reliably decomposed and removed, and the treated water W1 can be supplied to the subsequent treatment apparatus.
  • the applicant added a water-soluble bromide salt and hypochlorite to the water to be treated, and produced hypochlorite
  • a water treatment method having a urea decomposition step in which urea in the water to be treated is decomposed by bromate ions the free residual chlorine concentration in the effluent from the urea decomposition step is measured, and hypochlorous acid is added based on the measured value.
  • hypochlorous acid is added based on the measured value.
  • Patent Document 2 makes it possible to add the chemicals necessary for decomposing urea in just the right amount.
  • hypochlorite which is an oxidizing agent, is consumed, resulting in an insufficient amount of chemicals added for urea decomposition, and there is concern that urea may leak into the treated water. Understood.
  • the present invention has been made in view of the above problems, and includes adding a water-soluble bromide salt and hypochlorite to the water to be treated, and decomposing urea in the water to be treated with the generated hypobromite ions. Therefore, even if the component that consumes hypochlorite in the water to be treated fluctuates, the chemicals necessary for urea decomposition are added in just the right amount, and urea is stabilized and urea is stabilized without increasing the cost of urea treatment. It is an object of the present invention to provide a water treatment method and a water treatment apparatus that reliably removes impurities.
  • the present invention firstly provides water having a chemical addition mechanism comprising water-soluble bromide salt addition means and hypochlorite addition means provided in a supply channel of water to be treated.
  • a urea concentration measuring means provided upstream of the chemical addition mechanism, hypochlorite is added based on the chlorine consumption of the water to be treated, and the measurement result of the urea concentration measuring means is added.
  • the amount of extra hypochlorite to be added is determined based on the chlorine consumption of the water to be treated, and the amount of hypochlorite necessary for urea decomposition is determined based on the urea concentration contained in the water to be treated.
  • a chlorine demand measuring means of the water to be treated is provided in the preceding stage of the chemical addition mechanism, and the control means measures hypochlorite based on the measured value of the chlorine demand measuring means. It is preferable to add 0.1 to 10 mg/L (as available chlorine) of an acid salt (Invention 2).
  • the chlorine demand of the water to be treated as the raw water is measured by the chlorine demand meter, and the measured value of the chlorine demand and the measured value of the urea concentration measuring means are combined. feedforward control of the means for adding hypochlorite on the downstream side. Thereby, even if the water quality of the water to be treated fluctuates, urea can be stably treated by adding the water-soluble bromide salt and the hypochlorite in just the right amount.
  • the means for measuring the residual chlorine concentration of the water to be treated is provided upstream of the chemical addition mechanism, and the hypochlorite for pretreatment is added to the upstream side of the means for measuring the residual chlorine concentration.
  • the control means supplies hypochlorite from the pretreatment hypochlorite adding means so that the residual chlorine concentration of the water to be treated is 0.1 to 10 mg / L (as available chlorine) It is preferable to control the amount of chlorate added (invention 3).
  • the present invention provides a water treatment method in which a water-soluble bromide salt and hypochlorite are added to the water to be treated, and urea in the water to be treated is decomposed by the generated hypobromite ions, Before adding the water-soluble bromide salt and hypochlorite, add hypochlorite based on the chlorine consumption of the water to be treated, measure the urea concentration of the water to be treated, and measure the urea concentration.
  • a water treatment method is provided in which hypochlorite is further added based on the results (Invention 4).
  • the amount of hypochlorite to be added is determined based on the chlorine demand of the water to be treated, and the water-soluble bromide salt necessary for urea decomposition is determined based on the urea concentration contained in the water to be treated. and the amount of hypochlorite to be added, and by controlling the amount of hypochlorite to be added based on these, water-soluble bromide salts and hypochlorite can be added in just the right amount to stabilize urea.
  • the chlorine demand of the water to be treated is measured before adding the water-soluble bromide salt and hypochlorite, and hypochlorite is measured based on the chlorine consumption of the water to be treated. It is preferable to add 0.1 to 10 mg/L (as available chlorine) of an acid salt (Invention 5).
  • the chlorine demand of the water to be treated as the raw water is measured by the chlorine demand meter, and the measured value of the chlorine demand and the measured value of the urea concentration measuring means are combined. Based on this, by feed-forward controlling the amount of hypochlorite added on the downstream side, even if the water quality of the water to be treated fluctuates, water-soluble bromide salt and hypochlorite are added just enough to add urea can be stabilized.
  • the residual chlorine concentration of the water to be treated is measured before the water-soluble bromide salt and hypochlorite are added, and the residual chlorine concentration of the water to be treated is 0.1 to 10 mg. /L (as available chlorine) is preferably added to the water to be treated with hypochlorite for pretreatment (Invention 6).
  • inventions 4 to 6 it is preferable to control the amount of the water-soluble bromide salt added based on the measured value of the urea concentration (invention 7).
  • the water treatment apparatus of the present invention comprises means for measuring the concentration of urea provided upstream of means for adding water-soluble bromide salt and means for adding hypochlorite, and hypochlorite based on the amount of chlorine consumed in the water to be treated. and a control means for further adding hypochlorite from the hypochlorite addition means based on the measurement result of the urea concentration measurement means, so that the chlorine consumption of the water to be treated.
  • the amount of hypochlorite to be added is determined based on the amount, and the amount of water-soluble bromide salt and hypochlorite to be added required for urea decomposition is determined based on the concentration of urea contained in the water to be treated.
  • hypochlorite By controlling the amount of hypochlorite added based on the above, even if the water quality of the water to be treated fluctuates, water-soluble bromide salt and hypochlorite can be added just enough to stably treat urea. . Additionally, the chlorine demand may be measured by the DPD method.
  • FIG. 2 is a schematic diagram showing a water treatment device according to a second embodiment of the invention. It is a schematic diagram showing a conventional water treatment apparatus.
  • the ultrapure water production apparatus of the present invention will be described in detail below.
  • FIG. 1 shows a water treatment device according to a first embodiment of the invention.
  • This water treatment apparatus 1 includes a supply pipe 2 for raw water W as water to be treated, and sodium hypochlorite (NaClO) addition means 3 as hypochlorite provided in the middle of the supply pipe 2. and a sodium bromide (NaBr) addition means 4 as a water-soluble bromide salt are connected respectively, and these sodium hypochlorite addition means 3 and sodium bromide addition means 4 constitute a drug addition mechanism.
  • NaClO sodium hypochlorite
  • NaBr sodium bromide
  • a mixing device 5 and a reaction tank 6 are provided on the downstream side of this chemical addition mechanism, and a sodium bisulfite (NaHSO 3 ) addition means 7 as a reducing agent is connected to the downstream side of this.
  • W1 can be supplied to a post-treatment such as a primary pure water device.
  • a chlorine demand meter 9 and a urea meter 8 are provided on the upstream side of the sodium hypochlorite adding means 3 of the raw water W supply pipe 2 .
  • These chlorine demand meter 9 and urea meter 8, sodium hypochlorite adding means 3 and sodium bromide adding means 4 are connected to control means (not shown), respectively. Based on the measured value, the sodium hypochlorite adding means 3 and the sodium bromide adding means 4 can be controlled.
  • the chlorine demand meter 9 for example, one that can continuously measure the chlorine demand of ammonia nitrogen, iron, manganese, organic matter, etc. in a short time can be used. It may be one that quantifies and measures only nitrogen.
  • the chlorine demand of the raw water W is measured with the chlorine demand meter 9, and the control means responds to the indicated value (chlorine demand) from the sodium hypochlorite addition means 3.
  • the amount of sodium hypochlorite added at this time is generally 0.1 to 10 mg/L (as available chlorine).
  • the urea meter 8 measures the urea concentration of the raw water W, and based on this urea concentration, sodium hypochlorite is further added from the sodium hypochlorite addition means 3 by the control means, and from the sodium bromide addition means 4 Add sodium bromide.
  • the addition of sodium hypochlorite at this time may be performed by adding the total amount from one sodium hypochlorite addition means 3, or by providing a plurality of sodium hypochlorite addition means 3 (for example, two). , sodium hypochlorite corresponding to the chlorine demand and sodium hypochlorite for urea decomposition may be added.
  • hypobromite ions (BrO ⁇ ) generated from sodium bromide and sodium hypochlorite contributed to the decomposition of urea ((NH 2 ) 2 CO) and decomposed urea.
  • the subsequent bromide ions (Br ⁇ ) further react with hypochlorite ions (ClO ⁇ ) to become hypobromite ions (BrO ⁇ ) again and contribute to the decomposition of urea.
  • sodium hypochlorite is added in an amount corresponding to the chlorine demand based on the measured value of the chlorine demand meter 9, and urea is added based on the urea concentration of the urea meter 8.
  • the raw water W is generally tap water or industrial water whose source is river water or lake water. L or less, for example 20-60 ⁇ g/L.
  • the decomposition of urea by hypobromite ions generated by adding sodium bromide and sodium hypochlorite tends to progress relatively slowly, so the urea concentration is 10 ⁇ g /
  • the reaction vessel 6 it is preferable to secure the reaction vessel 6 for as long a reaction time as possible in the urea decomposition step. Specifically, it is preferable to secure a reaction time of about 4 to 10 hours.
  • a pure water production device or an ultrapure water production device can be suitably applied.
  • Sedimentation tank ⁇
  • Pretreatment equipment such as a filter, which consists of tanks, towers, pipes, pumps, etc., and is equipment that can obtain the desired reaction time and stirring effect. It may be substituted by imparting oxidant resistance (hypochlorous acid resistance, hypobromous acid resistance). More specifically, bromide salt and hypochlorite are added at the inlet of the raw water tank, the retention time of the entire pretreatment device is positioned as the reaction time, and the concentration of free chlorine at the outlet of the filter is adjusted to a predetermined value. Then, the addition of hypochlorite may be controlled, and the filter outlet water may be subjected to reduction treatment.
  • the water temperature of the raw water W in the water treatment method of this embodiment is preferably adjusted to 15 to 40°C, more preferably 20 to 30°C. This is because, in the above-mentioned urea decomposition reaction, as in general chemical reactions, under the same residence time conditions, the urea decomposition rate tends to decrease when the water temperature is low, and the urea decomposition rate tends to increase as the water temperature increases. has been confirmed. If the raw water W is tap water or industrial water, the water temperature may drop below 10°C in winter, so it is preferable to add a water temperature adjustment.
  • FIG. 2 shows an ultrapure water production system according to a second embodiment. Since the ultrapure water production apparatus 1 of this embodiment has basically the same configuration as the water treatment apparatus of the first embodiment described above, the same reference numerals are assigned to the same configurations, and detailed description thereof will be given. omitted.
  • the water treatment apparatus 1 includes sodium hypochlorite (NaClO) addition means 3 as a hypochlorite and sodium bromide (NaBr) addition as a water-soluble bromide salt to a supply pipe 2 for raw water W.
  • the sodium hypochlorite adding means 3 and the sodium bromide adding means 4 constitute a drug adding mechanism.
  • a mixing device 5 and a reaction tank 6 are provided on the downstream side of this chemical addition mechanism, and a sodium bisulfite (NaHSO 3 ) addition mechanism 7 as a reducing agent is connected to the downstream side of this.
  • W1 can be supplied to a post-treatment such as a primary pure water device.
  • the pretreatment hypochlorite addition means 11, the relay tank 12, the residual chlorine meter 13, and the urea meter 8 are provided upstream of the sodium hypochlorite addition means 3. are provided in this order.
  • These residual chlorine meter 13 and urea meter 8, sodium hypochlorite adding means 3, sodium bromide adding means 4 and pretreatment hypochlorite adding means 11 are each connected to control means (not shown). There is Then, based on the measured value of the residual chlorine meter 13, the pretreatment hypochlorite adding means 11 can be controlled, and based on the measured value of the urea meter 8, the sodium hypochlorite adding means 3 and sodium bromide addition means 4 can be controlled.
  • sodium hypochlorite is added to the raw water W from the hypochlorite addition means 11 for pretreatment, and retained in the relay tank 12 for a predetermined time. Consumed by reacting with contained ammonia nitrogen, iron, manganese, organic matter, etc. Then, the residual chlorine meter 13 measures the chlorine concentration of the raw water W flowing out of the relay tank 12 . At this time, the residual chlorine concentration is set in advance so that it can be judged that the chlorine demand is satisfied, and the control means controls the pretreatment level so that the measured value of the residual chlorine meter 13 is equal to or higher than this value (predetermined value). The amount of hypochlorite added from the chlorite adding means 11 is feedback-controlled.
  • the pretreatment hypochlorite adding means 11 so that the measured value (residual chlorine concentration) of the raw water W by the residual chlorine meter 13 is 0.1 to 10 mg / L (as available chlorine) It is preferable to control the amount of sodium hypochlorite added.
  • the urea meter 8 measures the urea concentration of the raw water W, the control means adds sodium hypochlorite from the sodium hypochlorite addition means 3 based on this urea concentration, and the sodium bromide addition means 4 adds odor. Add sodium chloride.
  • the sodium bromide and sodium hypochlorite are sufficiently mixed in the mixing device 5, and then retained in the reaction tank 6 for a predetermined time to cause a decomposition reaction of urea. to complete.
  • the chlorine concentration of the raw water W after adding sodium hypochlorite to the raw water W from the pretreatment hypochlorite adding means 11 is measured by the residual chlorine meter 13 , and feedback control is performed to add sodium hypochlorite from the pretreatment hypochlorite adding means 11 based on this measured value, so that hypochlorite based on the measured value of the urea meter 8 in the latter stage While optimizing the control of the amount of sodium hypochlorite added by the sodium hypochlorite addition means 3, stable urea decomposition treatment can be achieved.
  • the present invention has been described above based on the above-described embodiments, the present invention is not limited to the above-described embodiments, and various modifications are possible.
  • a general-purpose chemical injection pump, plunger pump, or the like is used as a method for adding chemicals from the sodium hypochlorite adding means 3, the sodium bromide adding means 4, and the pretreatment hypochlorite adding means 11, a general-purpose chemical injection pump, plunger pump, or the like is used.
  • a method of using a mixer such as a line mixer or a mixing reaction tank in combination can be used.
  • the post-treatment is not limited to pure water production equipment or ultrapure water production equipment, and can be applied to various equipment.
  • control of various adding means such as the sodium hypochlorite adding means 3, the sodium bromide adding means 4, and the pretreatment hypochlorite adding means 11 is manually controlled based on the measurements of various measuring instruments.
  • Example 1 Tap water having a urea concentration of 15 ⁇ g/L and an ammonia nitrogen concentration of 0.12 mg/L was prepared as raw water W.
  • This raw water W was supplied to the supply pipe 2, sodium hypochlorite was added as appropriate using a DPD reagent as a substitute for the chlorine demand meter 9, and the chlorine demand of the raw water W was measured. available chlorine). Therefore, after adding 1 mg / L (as effective chlorine) of sodium hypochlorite to raw water W, 3 mg / L of sodium bromide and 1.2 mg / L (as effective chlorine) of sodium hypochlorite were added. After stirring for 1 minute in the mixing device 5, the mixture was allowed to stand in the reaction tank 6 at a water temperature of 22° C. for 6 hours to decompose urea in the raw water W.
  • the urea concentration was less than 0.5 ⁇ g/L.
  • Example 1 In Example 1, 3 mg/L of sodium bromide and 1.2 mg/L of sodium hypochlorite (as available chlorine) were added to the raw water W, stirred for 1 minute with the mixer 5, and then the water temperature was 22° C. in the reactor. 6 for 6 hours to decompose the urea in the raw water W.
  • Example 2 In Example 1, 3 mg/L of sodium bromide and 4 mg/L of sodium hypochlorite (as available chlorine) were added to the raw water W, stirred for 1 minute with the mixer 5, and then added to the reaction vessel 6 at a water temperature of 22°C. After standing for 6 hours, the urea in the raw water W was decomposed.
  • the urea concentration of a sample of this treated water W1 was quantified by LC-MS analysis, the urea concentration was less than 0.5 ⁇ g/L, but compared with Experimental Example 1, it was 1.6 mg/L (as available chlorine ) of sodium hypochlorite becomes excessive. When 1.6 mg/L (as available chlorine) of sodium hypochlorite is reduced with sodium bisulfite, it is necessary to add about 2.2 mg/L excess sodium bisulfite.
  • Example 1 and Comparative Examples 1 and 2 above in the treatment of decomposing urea by adding a water-soluble bromide salt and hypochlorite based on the urea concentration, the water-soluble bromide salt and hypochlorite required for urea decomposition
  • the water-soluble bromide salt and hypochlorite required for urea decomposition
  • hypochlorite based on the chlorine demand of the raw water stable urea treatment can be achieved with the optimal amount of hypochlorite and reducing agent added. could be confirmed. Therefore, even if the urea concentration in the raw water W fluctuates, the chemical consumption can be reduced by changing the amount of hypochlorite to be added based on the chlorine demand of the raw water corresponding thereto.

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

Dans le dispositif et le procédé de traitement des eaux de l'invention, la demande en chlore de l'eau brute (W) est mesurée à l'aide d'un compteur de demande en chlore (9), et de l'hypochlorite de sodium correspondant à la demande en chlore est ajouté à partir d'un moyen d'ajout d'hypochlorite de sodium (3). En outre, la concentration d'urée dans l'eau brute (W) est mesurée à l'aide d'un compteur d'urée (8) et, sur la base de la concentration d'urée, de l'hypochlorite de sodium supplémentaire est ajouté à partir du moyen d'ajout d'hypochlorite de sodium (3) et du bromure de sodium est ajouté à partir du moyen d'ajout de bromure de sodium (4). Selon la présente invention, il est possible de fournir un procédé et un dispositif de traitement des eaux dans lesquels un agent chimique nécessaire à la dissolution de l'urée est ajouté sans excès ni déficit, même en cas de fluctuation des composants consommant des hypochlorites dans l'eau traitée, et dans lesquels l'urée est éliminée de manière stable et fiable.
PCT/JP2023/003009 2022-02-28 2023-01-31 Dispositif et procédé de traitement des eaux WO2023162593A1 (fr)

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JP2022-029105 2022-02-28
JP2022029105A JP7351362B2 (ja) 2022-02-28 2022-02-28 水処理装置及び水処理方法

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011183245A (ja) * 2010-03-04 2011-09-22 Kurita Water Ind Ltd 超純水製造方法及び装置
JP2019063768A (ja) * 2017-10-04 2019-04-25 栗田工業株式会社 水処理方法及び水処理装置
JP2022002830A (ja) * 2020-06-23 2022-01-11 オルガノ株式会社 純水製造装置及び純水製造方法
JP2022030031A (ja) * 2020-08-06 2022-02-18 オルガノ株式会社 純水製造装置及び純水製造方法
JP2022081825A (ja) * 2020-11-20 2022-06-01 オルガノ株式会社 尿素処理方法及び装置

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011183245A (ja) * 2010-03-04 2011-09-22 Kurita Water Ind Ltd 超純水製造方法及び装置
JP2019063768A (ja) * 2017-10-04 2019-04-25 栗田工業株式会社 水処理方法及び水処理装置
JP2022002830A (ja) * 2020-06-23 2022-01-11 オルガノ株式会社 純水製造装置及び純水製造方法
JP2022030031A (ja) * 2020-08-06 2022-02-18 オルガノ株式会社 純水製造装置及び純水製造方法
JP2022081825A (ja) * 2020-11-20 2022-06-01 オルガノ株式会社 尿素処理方法及び装置

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